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Method for synthesizing star-shaped solution polymerized butadiene-styrene rubber by using modified initiator

A technology of solution polymerization of styrene-butadiene rubber and initiator, applied in the field of rubber, can solve the problems of high rubber Mooney viscosity, high price of raw materials, and lack of compatibility of carbon black, so as to save production costs, improve production efficiency, and shorten polymerization time Effect

Inactive Publication Date: 2011-07-13
BEIJING UNIV OF CHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Equally, the preparation of this initiator faces the disadvantages of high raw material price, complex preparation process, and needs to be carried out in polar solvents, and the synthesized rubber Mooney viscosity is relatively high.
[0006] The problem in the above method is either to reduce the number of free ends, to modify one end of the solution polystyrene butadiene rubber macromolecular chain to obtain a star polymer, but the other end is not modified; or to improve the combination with additives Based on the ability to modify the two ends of the linear polymer, but the modified group either has no compatibility with carbon black, or the preparation of the modified initiator is difficult and the process is complicated

Method used

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  • Method for synthesizing star-shaped solution polymerized butadiene-styrene rubber by using modified initiator
  • Method for synthesizing star-shaped solution polymerized butadiene-styrene rubber by using modified initiator
  • Method for synthesizing star-shaped solution polymerized butadiene-styrene rubber by using modified initiator

Examples

Experimental program
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Effect test

Embodiment 1

[0042] Under nitrogen protection, add 80ml of cyclohexane, 25mmol of 1,1-diphenylethylene, and 25mmol of n-butyllithium into a purified 250ml polymerization bottle with electromagnetic stirring, and react at 40°C for 80 hours to obtain Modified initiator I-1 shown in structural formula I.

[0043] Under nitrogen protection, add 77ml of cyclohexane, 7.8g of butadiene, and 0.96ml of tetrahydrofuran into a purified 250ml polymerization bottle, take 0.39mmol of the modified initiator I-1 synthesized above, and react at 55°C for 3 hours The reaction was terminated with methanol, and the product was dissolved in cyclohexane, then flocculated with ethanol, then ultrasonically cleaned three times with ethanol, and vacuum-extracted and dried. Linkage with gel permeation chromatography (GPC)-ultraviolet detector, record the number average molecular weight of product polybutadiene to be 22000, as figure 1 . pass figure 1 It can be seen that the characteristic absorption peak of the be...

Embodiment 2

[0045] Under the protection of nitrogen, add 70ml of cyclohexane, 20.2ml of tetrahydrofuran, 25mmol of 1,1-diphenylethylene, and 25mmol of n-butyllithium into a purified 250ml polymerization bottle with electromagnetic stirring, and react at 55°C for 40 Hours, the compound I-2 shown in structural formula I was obtained.

[0046] Under the protection of nitrogen, add 80ml of cyclohexane, 6.4g of butadiene, 1.6g of styrene, and 0.42ml of tetrahydrofuran into a purified 250ml polymerization bottle, and take 0.13mmol of the modified initiator I-2 synthesized above, at 55°C After 3 hours of reaction, the reaction was terminated with methanol, and the product was vacuum-extracted, and the number-average molecular weight of the product measured by GPC and nuclear magnetic resonance was 67,000, the styrene content was 19.8%, and the vinyl content was 49.5%.

Embodiment 3

[0048] Under nitrogen protection, add 100ml of cyclohexane, 30mmol of 1,1-diphenylethylene, and 30mmol of sec-butyllithium into a purified 250ml polymerization bottle with electromagnetic stirring, and react at 40°C for 70 hours to obtain Compound I-3 shown in structural formula I.

[0049] Under nitrogen protection, add 120ml of cyclohexane, 9.0g of butadiene, 3.0g of styrene, and 0.81ml of tetrahydrofuran into a purified 250ml polymerization bottle, and take 0.2mmol of the modified initiator I-3 synthesized above, at 55°C After reacting for half an hour, raise the temperature to 60°C for 1 hour, add SnCl 4 0.056 millimoles were used for the post-coupling reaction. After 2 hours of reaction, the reaction was terminated with methanol solution to obtain the product. The number-average molecular weight was 125,000, the styrene content was 24.6%, and the vinyl content was 46.3%.

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Abstract

The invention discloses a method for synthesizing star-shaped solution polymerized butadiene-styrene rubber by using modified initiator, belonging to the technical field of rubber. The method comprises the following steps: synthesizing a compound I; using the compound I as initiator and Lewis base as structural modifier and randomizer to perform the random copolymerization of butadiene and styrene in hydrocarbon solvent under the protection of nitrogen; and after the copolymerization reaction, adding coupling agent to perform c oupling reaction, stopping the reaction, and performing condensation to obtain the modified star-shaped solution polymerized butadiene-styrene rubber. One end of the rubber has a star-shaped structure through coupling modification, thus the number of free ends can be greatly reduced; the other end has a benzene ring brought by the initiator, thus the affinity to carbon black can be improved; and compared with the unmodified solution polymerized butadiene-styrene rubber, the solution polymerized butadiene-styrene rubber prepared by the method has low rolling resistance, good wet skid resistance and excellent physical and mechanical properties.

Description

technical field [0001] The invention belongs to the technical field of rubber, and relates to a method for synthesizing star-shaped solution-polymerized styrene-butadiene rubber with a modified anionic polymerization initiator, in particular to better modification of the terminal group of solution-polymerized styrene-butadiene rubber by modifying the initiator , the solution-polymerized styrene-butadiene rubber has low rolling resistance and good wet skid resistance. Background technique [0002] The fuel consumption caused by tires accounts for about 20% of the fuel consumption of the entire car, and in trucks, this ratio increases to 1 / 3. In recent years, due to the pressure of energy resources and the environment, people have put forward higher and higher requirements for the energy saving, safety and comfort of automobile tires, so the concept of green tires has gradually attracted people's attention since the 1990s. Compared with traditional tires, due to the applicati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F236/10C08F4/48C08F8/42
Inventor 张兴英陈波赵素合白玉徐利民
Owner BEIJING UNIV OF CHEM TECH
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